Process for dewaxing oil



40 wax to settle to the Patented Oct. 3, 1939 UNITED STATES PATENT OFFICE PROCESS FOR DEWAXING OIL Original application July 17, 1933, Serial No.

Divided and this application February 25, 1936, Serial No. 65,627

3 Claims.

This invention relates to wax separation ,irom wax bearing oil, and is a division of our copending application Serial No. 680,710 which was filed July 17, 1933, and has matured into Patent Num- 5 ber 2,053,552. This invention relates more particularly to the separation of precipitated Wax from suspension in oil.

Many crude oils from which lubricating oil is produced contain paraffin or wax. It is found associated with lubricating oil fractions of paraffln base crude oil, asphalt base crude oil and mixtures or blends of lube oil fractions of hot paraflin and asphalt base crude oils. The wax is not only of doubtful lubricating value but limits the minimum temperature at which lubricating oils containing it can be used, by congealing at low temperatures. Therefore, in the production of lubricating oil from petroleum fractions containing wax or parafiin, it is customary to remove a substantial portion of the wax or paraflin present in the oil in order to lower its po;.1r point or the temperature at which it com ea s.

The separation of wax from wax bearing lubrieating oil fractions has been accomplished by several processes in the past, the two most commom and oldest of which are the cold settling process-and the cold pressing process.

In the cold settling process" the wax-containing oil is first diluted with a quantity of a light hydrocarbon fraction, such as naphtha, gasoline, or kerosene. The diluted wax-containing oil is then slowly chilled by suitable refrigerating means for a period of 20 to 50 hours until a 35 temperature is reached which corresponds to the desired pour point portion of the wax is precipitated. The chilled oil and precipitate mixture is then allowed to stand for a period of several weeks to allow the bottom of the chilling tank. Objections to this process are the cost of refrigeration for the necessary long periods of time, the large capacity of refrigeration and storage equipment, and the poor separation of wax and oil obtained.

In the cold pressing process the wax-containing oil is chilled slowly as in the above described cold settling process. The chilled mixture of precipitated wax and oil is then pumped through a filter press under a pressure of 300 to 350 pounds per square inch. The wax precipitate is collectedupon the filter and the oil is removed as a pressed distillate relatively free from wax. This process has found commercial application only in conjunction with oil having and atwhich a substantial wax present in a crystalline form. Amorphous and/or micro-crystalline wax has been found extremely diflicult and impracticable to separate by filtration methods.

Objects of this invention are to overcome the enumerated disadvantages and other disadvantages of the common wax separation methods, and to provide a novel process for separating wax from oil which will be eflicient, economical, of higher capacity, and less costly in time and equipment than the processes heretofore employed.

Other objects are to provide a process for separation of precipitated wax from wax-bearing oil which will be complete, in which the time of settling and separation of the wax is greatly reduced, and in which the time and energy consumption of refrigeration is a minimum, and by which fine precipitates both crystalline and amorphous can be successfully separated. Another object of this invention is to provide a -method wherein wax can be separated from waxbearing oil which has been quickly cooled or shock chilled. Another object of the invention is to providea process employing electrical trea ment of the wax-bearing oil wherein the rate of cooling of the said wax-bearing oil can be greatly increased and the time for settling and separation greatly reduced.

In general these objects are attained according to the invention through treating the mixture of oil and precipitated wax by electrical field or current.

The invention is embodied in apparatus capable of performing a process comprising chilling a wax-bearing oil or a solution of such an oil in a suitable diluent to a temperature at which wax preciptation therein takes place, subjecting the diluent, oil and wax precipitate solution or mixture to an electric field or electric current to aid separation, and depositing and settling, filtering and/or centrifuging the thus treated oil to further separate the wax therefrom.

The invention broadly stated comprises a method of treating wax-bearing oil with an electric field or current to aid separation of wax therefrom. The invention more specifically stated comprises a process for treating waxbearing oil and/or wax-bearing oil containing precipitated wax, by an electrical field or current to aid in separation and deposition of the precipitated wax, to reduce the time of chilling and settling and to increase the efficiency and completeness of separation y subsequent separating methods.

Other objects and advantages and features of the invention will be evident hereinafter.

The accompanying drawing illustrates one embodiment of the invention. I

Wax-bearing oil at a temperature above that at which wax is precipitated from solution is stored in tank II]. This oil is withdrawn from the tank II] by pump l2 and forced through line l3 and valve M to a mixer l5 where it meets and dissolves in a stream of a light hydrocarbon diluent supplied through line is and valve lid from diluent storage tank H. The solution of waxcontaining oil and diluent passes from mixer it through line l9 into refrigerator 2t! where'it is chilled to a temperature at which a substantial amount of wax is precipitated from solution. The mixture of wax-bearing oil, diluent and precipitate flows through valve 22 into the treater chamber 25 where it is subjected to an electric field. The electric treating field is established between a central electrode ill and the treater chamber wall 28, the electricalpotential therefor being supplied by generator til. Suitable electrical connections 3t and iii are provided from generator 29 to the said central electrode through high tension lead-in insulator 32 to the treater wall.

The wax precipitate which settles to the bottom of treater chamber 25 may be withdrawn through outlet it by means of pump 35 and expelled through valve 36. The solution from which a portion of wax has thus been removed is decanted from the top portion of the treater'chamber through line 38 and allowed to how through line 39, valve Ml, line 42 and valve tie into a separating tank 5b where a substantial portion of the remaining precipitated wax is allowed to settle out. The wax which settles to the bottom oi settling tank 5% is withdrawn through outlet 52 by means of pump 53 and'expelled through valve 54.

The solution from which the wax has been separated is withdrawn from the top of the settling tank through line b, valve 5d and introduced into still $6 through line at where the diluent is distilled from the oil.

Heat for distillation is supplied by means of heating coil El.

The oil bottoms from which the diluent has been distilled is withdrawn from still dd through outlet valve 53 and run to the dewaxed oil storage tank through line 64.

The vapors from the top of stilltt are withdrawn through vapor line 58 and condensed in condenser 59 and the condensate returned by means of pump 50 through line 6! to the diluent storage tank H.

. In some cases it is desirable instead of expelling the settlings from the treater chamber 25 through valve 36 to run it to the separator 50 for further settling and separation. In this case, valves 36, 40 and 45 are closed and valve 4% opened and the said settlings are forced bytmeans of pump 35 through line 44, valve 4|, line 42 and valve 43 into the separator 50. The solution from which the wax has been partially removed may then be withdrawn from the top of the treater chamber 25 through outlet 38, valve- 31 and forced by means of pump 46 to a filter press 41.

The filtrate from filter press 41 may be'introduced into the still through line 48, valve 49 and inlet 51. A centrifuge or any other means for separating precipitated wax may be substituted for the filter press 41 if desired.

In some cases it is also desirable to run the wax precipitate settlings from treater chamber 25 to the filter press 41 and this is accomplished by closing valves 36, 3t and 4| and forcing said settlings by means of pump 35 through line 44 and valve 45 to pump 46 and from there to said filter press 41. Recirculation of the solution in treater chamber 25 may be accomplished with pump 35 by closing valves iii, 33 and 45 and. opening valves db and ll.

A battery of electric treater chambers, such as illustrated in the drawing by numeral 25, may be employed in parallel and valve 24 and branch line it from the refrigerator idare provided for naliing connection with them. With this arrangement the operation of the electric treating chambers may be alternated to allow the precipitated wax, which has accumulated upon the electrode and the treater chamber surfaces, to be removed and the inside of the chamber thoroughly cleaned. For continuous operation suitable mechanical means, such as scrapers, may be employed for removing deposited wax from the electrode and the chamber surfaces.

As an example or" the operation of this method of dewaxing oil a 27% solution of wax in a light hydrocarbon was chilled to a temperature at which a substantial portion of this wax was precipitated from. solution and the resulting mixture was treated by a high potential direct current for a period of fifteen minutes. At the end of this time the electrodes were found to be heavily coated with precipitated wax. It has been found that the portion oi the wax which is not deposited on the electrodes duringelectrical treatment is agglomerated and the precipitate thus treated is in a form which can be much more readily settled or otherwise separated as by filtration or centrifuging.

It is desirable in some cases to dilute the waxbearingoil with a diluent, chill the solution to a point where wax precipitates from solution, separate a portion of the war; from the chilled solution by settling and subsequently treat the chilled solution electrically to separate the remaining wax not removed by the prior settling.

I Naphtha, gasoline, liquid propane, acetone and benzol, methyl chloride, halogenated hydrocarbons, such as monochloro- -difiuoro methane. dichloro -difiuoro methane, dichlorethylene, trichlorethylene, or others or mixtures of ethers and alcohols may be employed as diluents for the wax-bearing oil.

Potential gradients of 5,0(ld to 35,000 volts per ,inch either continuous or interrupted direct current through the solution have been found eflective in agglomerating and depositing the precipiptated wax. Some waxes appear to be negatively charged and to show a tendency to deposit most heavily on the positive electrode. When it is desired to agglomerate the wax particles without deposition, to aid settling and separation or filtering or-centrifuging, analternating potential is effective. a

An advantage of the present process is that the oil solution containing wax can be shock chilled and bymeans of electrical treatment good separation and settling obtained. Heretofore with conventional methods of wax separation, very slow cooling of the waxy solution over long periods of time was required.

' The process is not limited to the treatment of wax but is applicable to asphalt, asphaltines, petrolatum, sludges and other substances both solid and plastic, r

hill

It is to be understood that the foregoing is merely illustrative of one apparatus and method and that the invention is not limited thereby but may include any method and apparatus which acccmplishes the same within the scope of the invention.

We claim:

1. A process for the separation of wax from a wax-bearing oil which comprises shock chilling said oil to precipitate wax, subjecting the chilled oil containing precipitated wax to the influence of an electric field between electrode surfaces immersed therein to form wax which is readily separable in character and separating the wax from the chilled mixture by electro-deposition upon an immersed electrode surface in said chilled mixture.

2. A process for the separation of wax from wax-bearing oil which comprises quickly cooling and thereby shock chilling wax-bearing oil to precipitate the wax therein, subjecting the thus chilled oil and wax mixture to the influence of an electric field between electrodes, and separating the wax from the chilled mixture by electrodeposition upon an electrode.

3. A process for the separation of wax from wax-bearing oil which comprises shock chilling said oil by quickly cooling the oil, thereby precipitating wax in the oil, subjecting the chilled oil containing the precipitated wax to the infiuence of an electric field between electrodes to modify the form of the wax, and separating the wax from the chilled mixture by electro-deposition upon an electrode while under the influence of an electric field.

' LYLE DILLON.

CLAUDE E. SWIFT. 

